• Title/Summary/Keyword: ether extraction

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A Study on the Extraction of Monasil PCA using Liquid CO2 (액체 이산화탄소 이용한 Monasil PCA 추출에 대한 연구)

  • Cho, Dong Woo;Oh, Kyoung Shil;Bae, Won;Kim, Hwayong;Lee, Kab-Soo
    • Korean Chemical Engineering Research
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    • v.50 no.4
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    • pp.684-689
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    • 2012
  • Poly(acrylic acid) (PAA) microspheres is one of the widely-used polymeric materials for the bio-field application and the electric materials. For the synthesis of PAA microspheres, the polymerization technique using surfactants is applied. After the synthesis, the purification and separation processes are required for the removal of surfactant. When general organic solvents were used, many problems, such as huge amount of waste solvent, additional separation processes, and the possibility of residual media, were occurred. Thus, High-pressure Soxhlet extraction using liquid $CO_2$ was developed to solve these problems. In this study, High-pressure Soxhlet extraction of the synthesized PAA microspheres using liquid $CO_2$ was conducted for the removal of Monasil PCA which is used for the dispersion polymerization of acrylic acid in compressed liquid Dimethyl ether (DME). The morphology of the extracted PAA particles was checked by field emission scanning electron microscopy (FE-SEM) and the residual concentration of Monasil PCA was analyzed by inductively coupled plasma - Optical Emission Spectrometer (ICP-OES). For studying the effect of the solvent effect, Soxhlet extraction was conducted using n-hexane, liquid DME, and liquid $CO_2$. In case of n-hexane, some extracted PAA microspheres were produced. However, deformation was also occurred due to the high thermal energy of n-hexane vapor. Liquid DME could not remove Monasil PCA. When using liquid $CO_2$, the extracted PAA microspheres which were free for the residual solvent were produced without deformation. For finding the optimum operating condition, high-pressure Soxhlet extraction was conducted for 8 hours with changing the temperature of reboiler and condenser. When the extractor temperature is $19.6{\pm}0.2^{\circ}C$ and the pressure is $51.5{\pm}0.5$ bar, the best removal efficiency was obtained.

Biodegradation of Kraft Lignins by White-Rot Fungi(I) -Lignin from Pitch Pine- (백색부후균에 의한 크라프트 리그닌의 분해(I) -리기다소나무 리그닌-)

  • 김명길;안원영
    • Journal of Korea Foresty Energy
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    • v.17 no.1
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    • pp.56-70
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    • 1998
  • This study was carried out to investigate the structural characteristics of kraft lignin and the wood degrading characteristics, the productivity of ligninolytic enzymes and the enzymatic degradation of kraft lignin by white-rot fungi. To purify kraft lignin, precipitation of kraft pulping black liquors of pitch pine meal was done by titration with lN $H_{2}SO_{4}$ reaching to pH 2, and isolation of the precipitates done by centrifugation. The isolated precipitates from pitch pine were redissloved in lN NaOH, reprecipitated by titration with lN $H_{2}SO_{4}$, washed with deionized water, and kept ofr analysis after freeze drying. Fractionation of the precipitates in solution by successive extraction with $CH_{2}Cl_{2}$ and MeOH, and the fractionates were named SwKL, SwKL I, SwKL II, and SwKL III for pitch pine kraft lignin. The more molecular weights of kraft lignin increased, the less phenolic hydroxyl groups and the more aliphatic hydroxyl groups. Because as the molecular weights increased, the ratio of etherified guaiayl/syringyl(G/S ratio) and the percentage were increased. The spectra obtained by 13C NMR and FTIR assigned by comparing the chemical shifts of various signals with shifts of signals from autherized ones reported. The optimal growth temperature and pH of white-rot fungi in medium were $28^{\circ}C$ and 4.5-5.0, respectively. Especially, in temperature and pH range, and mycelial growth, the best white-rot fungus selected was Phanerochaete chrysosporium for biodegradation. For the degradation pathways, the ligninolytic fungus jcultivated with stationary culture using medium of 1% kraft lignin as a substrate for 3 weeks at $28^{\circ}C$. The weight loss of pitch pine kraft lignin was 15.8%. The degraded products extracted successively methoanol, 90% dioxane and diethyl ether. The ether solubles were analyzed by HPLC. Kraft lignin degradation was initiated in $\beta$-O-4 bonds of lignin by the laccase from Phanerochaete chrysosporium and the degraded compounds were produced from the cleavage of $C\alpha$-$C\beta$ linkages at the side chains by oxidation process. After $C\alpha$-$C\beta$ cleavage, $C\alpha$-Carbon was oxidized and changed into aldehyde and acidic compounds such as syringic acid, syringic aldehyde and vanilline. And the other compound as quinonemethide, coumarin, was analyzed. The structural characteristics of kraft lignin were composed of guaiacyl group substituted functional OHs, methoxyl, and carbonyl at C-3, -4, and -5 and these groups were combinated with $\alpha$ aryl ether, $\beta$ aryl ether and biphenyl. Kraft lignin degradation pathways by Phanerochaete chrysosporium were initially accomplished cleavage of $C\alpha$-$C\beta$ linkages and $C\alpha$ oxidation at the propyl side chains and finally cleavage of aromatic ring and oxidation of OHs.

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High-Purity Purification of 2,6-Dimethylnaphthalene (2,6-DMN) in Light Cycle Oil - Purification of 2,6-DMN from Concentrate of DMN Isomers by Crystallization - (접촉분해경유 중의 2,6-dimethylnaphthalene (2,6-DMN)의 고순도 정제 - 결정화에 의한 DMN 이성체 농축액 중의 2,6-DMN의 정제 -)

  • Kim, Su Jin;Jeong, Hwa Jin
    • Applied Chemistry for Engineering
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    • v.19 no.1
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    • pp.105-110
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    • 2008
  • The high-purity purification of 2,6-dimethylnaphthalene (2,6-DMN, 10.43 wt%) from the concentrate of DMN isomers recovered from light cycle oil (LCO) through distillation-extraction combination was examined by a crystallization operation. To select the most suitable crystallization solvent for purification of 2,6-DMN, several conventional solvents, which have been employed commercially as crystallization solvents for high-purity performance, were tested, through measurement of purity and yield of 2,6-DMN. The solvents used were acetone, cyclohexanone, ethanol, ethyl ether, ethyl acetate, isopropyl ether, methanol, n-hexane, n-heptane, pyridine, THF, toluene, and a mixture of methanol and acetone. The mixture of 60 vol% methanol and 40 vol% acetone (M/A = 1.5) was found to be suitable for purification of 2,6-DMN in the concentrate of DMN isomers based on purity and yield. Increasing the operation temperature and the volume ratio of solvent (M/A = 1.5) to feed (concentrate of DMN) resulted in improving the purity of 2,6-DMN, whereas the yield decreased. The crystal recovered by crystallization run using the concentrate of DMN isomers contained about 76 wt% 2,6-DMN. Furthermore, for recovery of high-purity 2,6-DMN, crystal containing 76 wt% 2,6-DMN was crystallized. As a result, crystal with 99.7 wt% 2,6-DMN was recovered with 40% yield.

Studies on the Development of Hydrangea and Stevia as a Natural Sweetening Products (천연감미료(天然甘味料) 자원식물(資源植物) Hydrangea 및 Stevia의 개발(開發)에 관(關)한 조사연구(調査硏究))

  • Chung, Myung-Hyun;Lee, Myung-Yul
    • Korean Journal of Pharmacognosy
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    • v.9 no.3
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    • pp.149-156
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    • 1978
  • The result of the study about the cultivation, the constituents, the sweetenity, and the development of preparations of Stevia and Hydrangea are as follows: 1. Hydrangea thrived at $200{\sim}1,400m$ above the sea-level, and the good ones were brought up at $600{\sim}1,200m$. 2. The good ones which belonged to the genera of Hydrangea were produced in the damp, dark and cold place. 3. The growth and cultivated yield of Stevia was not significantly influenced by the acidity of the soil. 4. The best season was May and June for propagation of Stevia by cutting method. 5. The growth rate of Stevia and Hydrangea was really good in the sandy fertile soil, but in the mucotic soil it was not suitable. 6. The extraction and separation of phyllodulcin by solvent had many difficulties, because it was very soluble in water, ethanol, ether, petroleum ether, acetone and benzene, etc. 7. The solubility of stevioside on the solvent was as follows: It was very soluble in water and methanol, slightly soluble in ethanol and acetone, and insoluble in ether, petroleum ether and chloroform. 8. The alkaloid reaction by Mayer reagent in Hydrangea extract was positive. 9. The ashification rate of Stevia was 8.66% to 8.72% and that of Hydrangea 17.02% to 17.04%. 10. The tannin of Stevia leaf was 7.80% to 7.88% and its of Hydrangea decreased 9.46% to 6.08% by fermentation. 11. The percent rates in minimum concentration-occurring sweetness in sugar, glycyrrhiza methanol extract, Hydrangea water extract, Stevia leaf water extract, decoction of Stevia's leaf, decoction of Stevia's stem were as follows: 1.2, 0.1, 0.1, 0.2, 0.4, 0.01, 0.1, 0.6. and sweetenity ratios of those were 1, 12, 12, 6, 3, 64, 12, 2, 12. It was very meaningful to develop preparations of stevia as stevioside, micronized powder, water extract, methanol extract and compound teas and in Hydrangea, water extract, methanol extract, single tea, and compound teas were less meaningful. 13. The genera of Hydrangea which is natural species in Korea was positive in phyllodulcin-identification test, but it was not available to make the sweet tea because of having a little content.

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Improvement of Determination Method for Propionic Acid in Bakery Products (빵의 프로피온산 함량 분석방법 개선)

  • Lee, Sung-Deuk;Kim, Yeon-Sun;Doo, Ok-Joo;Kim, Mi-Sun;Park, Young-Hae;Kim, Il-Young;Chae, Young-Zoo
    • Journal of Food Hygiene and Safety
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    • v.24 no.4
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    • pp.332-337
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    • 2009
  • Most propionic acid is added to food (especially breads) as preservatives and its form is sodium or calcium salt. Most countries admitted propionic acid as food preservatives but a tolerance limit is somewhat different according to countries. Recoveries of the official method for propionates reported as 50.0~60.0%. Accordingly new rapid determination method for propionates was developed using formic acid added sodium chloride (5 g) and ether (formic acid : ether = 1 : 2) as the extraction solvent to improve the official method with the complex processes. Propionate was dissolved from the samples with formic acid omitting steam distillation and ion exchange procedure. Then propionate in formic acid was extracted with ether and sodium chloride again. A $1\;{\mu}l$ aliquot of the filtrate of ether was analyzed by gas chromatograph. Recoveries from sample A and B fortified with propionic acid sodium salt were 85.0 % and 90.0 %, respectively.

A Study on Capillary Gas-Liquid Chromatographic Determination of Diosgenin in Costus Speciosus (모세관 기체-액체 크로마토그래피에 의한 Costus Speciosus 중 Diosgenin의 정량에 관한 연구)

  • Taek Jae Kim;Cha Kee Surk;Kim Young Sang
    • Journal of the Korean Chemical Society
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    • v.30 no.4
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    • pp.369-376
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    • 1986
  • Diosgenin in an Indonesian Costus speciosus was determined by capillary gas-liquid chromatography (GLC). The experimental conditions for the hydrolysis, extraction and acetylation of the diosgenin, and the determination by GLC were investigated. 0.20g of dried sample powder was refluxed in the solution of 3N HCI and xylene at 95∼100${\circ}C$ for 4 hours and the xylene layer was separated. The residue evaporated the xylene was refluxed in 20 : 80 acetic anhydride-pyridine for 30 minutes and the diosgenin acetate was extracted with diethyl ether. Dehydrated with anhydrous $Na_2SO_4$ and evaporated the ether, the residue was dissolved in 5.00ml of n-hexane and injected into GLC. Capillary column of SE-30 25m ${\times}$ 0. 33mm was installed in GLC and the column temperature was increased from 180${\circ}$ to 270${\circ}C$ at rate of 10${\circ}C$/min. The flow rate of carrier gas $N_2$ was 2ml/min and FID was used to detect. The analytical result of the diosgenin was 0.281% and relative standard deviation of 5 measures was 1.8%.

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Effects of Ulva lactuca Extracts on Cytotoxicity of Cancer Cell Lines and Immune Stimulation (갈파래(Ulva lactuca) 추출분획의 암 세포주에 대한 세포독성 및 면역활성 효과)

  • Jang, Min-Kyung;Kim, Nam-Young;Lee, Dong-Geun;Lee, Jae-Hwa;Ha, Jong-Myung;Ha, Bae-Jin;Kim, Mi-Hyang;Bae, Song-Ja;Jang, Jeong-Su;Lee, Sang-Hyeon
    • Journal of Life Science
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    • v.16 no.7 s.80
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    • pp.1169-1173
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    • 2006
  • Extracted fractions of the green seaweed Ulva lactuca were studied to verify the cytotoxicity and immunostimulating activity. The fractions from the ethanol extract of U. lactuca were prepared by the systematic extraction procedure with solvents such as hexane, ethyl ether, methanol, butanol and $H_2O$. The cytotoxic effects of U. lactuca fractions against human leukemia cell line U937, mouse neuroblastoma cell line (NB41A3), human hepatoma cell line (HepG2) and rat glioma cell line (C6) were investigated. Ethyl ether fraction showed the highest cytotoxicity against all four cell lines tested. In addition, $H_2O$ fraction also showed relatively high cytotoxicity. Dose dependent patterns were observed on all four cell lines. The immune-stimulating effects of U. lactuca fractions on rat macrophage cell line (RAW 264.7) were also investigated. All five fractions of U. lactuca extract stimulated NO production with concentration dependant manner. These results suggest that U. lactuca may be a useful candidate for a natural cancer preventing and immune-stimulating agents.

Antimicrobial Activity of Clove Extract by Extraction Solvents (용매별 정향 추출물의 항균활성)

  • 이옥환;정승현;손종연
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.33 no.3
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    • pp.494-499
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    • 2004
  • This study was investigated the antimicrobial activity of clove extracts according to extraction solvents. The extracts were tested for their antimicrobial activity against several food spoilage microorganisms including Bacillus subtilis, Staphylococcus aureus, Escherichia coli, Salmonella typhimurium and Pseudomonas aeruginosa. The methanol extract showed stronger antimicrobial activities than water extract. However, petroleum ether extract did not show antimicrobial activity. The water extract of clove showed growth inhibition effect against Escherichia coli, Salmonella typhimurium and Staphylococcus aureus, whereas no effect against Bacillus subtilis. The methanol extract of clove extracts showed more sensitive antimicrobial activity in Gram (+) bacteria than in Gram (-) bacteria. The antimicrobial activities were increased with increasing concentration of the clove extract.

Separation and Composition of Sesame Meal Protein (참깨박(粕) 단백질(蛋白質)의 분리(分離)와 조성(組成))

  • Kim, Jun-Pyong;Shim, Woo-Man;Kim, Chong-Ik
    • Applied Biological Chemistry
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    • v.23 no.1
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    • pp.14-22
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    • 1980
  • White and black sesame produced in Korea were defatted with ethyl ether or n-hexane. Defatted sesame meal was extracted with water and salt solution, and protein extraction was precipitated at various pH 1 through 12, with trichloro acetic acid (TCA), tannic acid and ammonium sulfate, respectively. Protein was purified by Sephadex A-25, G-75, G-100 and G-200, and identified its protein fraction by polyacrylamide gel electrophoresis. Amino acids composition of protein in white sesame was analyzed by automatic amino acid analyzer. Protein contents of white sesame, black sesame and sesame meal are 20.5%, 19.2%, and 44.7%, respectively. n-Hexane was the most suitable solvent for extraction of oil from sesame. Crude protein precipitation was better in higher pH. The protein extraction was more effective with the solution containing sodium chloride tinder the pH 8. Globulin in total protein was high and prolamin was less than in other cereal proteins. Glutamic acid contents of white sesame and sesame globulin were 17.1%, and 20%, respectively. Both proteins contained relatively high levels of essential amino acids. 12-13 bands were found in water soluble protein and 2 bands in salt soluble protein were detected by the disc gel electrophoresis, and were identified in both of white and black sesame. The salt soluble protein of white sesame could be purified by Sephadee G-100 and G-200.

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Convenient Methods for the Extraction and Discrimination of Water-Soluble Plant Pigments (수용성 식물 색소 추출 및 판별에 관한 간편한 방법)

  • Chung, Sang-Ho;Byun, Young-Ho
    • The Journal of the Korea Contents Association
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    • v.9 no.3
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    • pp.353-360
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    • 2009
  • The use of colorants as additives for foods and drinks is a significant factor to food consumers in determining the acceptability of processed foods. In recent years, the number of previously used artificial colorants/dyes suitable for food use has been drastically reduced as a result of toxicological studies. Therefore, the use of natural pigments such as anthocyanins and betacyanins that were known to have anticancer and antioxidant activities is increasingly required. In this study, the water-soluble plant pigments, anthocyanins and betacyanins, were easily extracted with a very simple method using a few organic solvents such as ethyl acetate, ethyl ether, and chloroform. After the extraction of them, these two major plant pigments could be also simply and rapidly separated and discriminated by a solely one-stepped agarose gel electrophoresis in a citrate buffer (pH 3.0).